Ethyl Acetate → HCID 73656239, Verbindung

HRID 1885737Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1885737
[Cl:1][C:2]1[CH2:3][N:4]=[CH:5][C:6]2([CH3:21])[CH:17]([CH3:18])[CH:15]3[CH2:16][C:10]4=[C:11]([N:14]3C#N)[CH2:12][CH2:13][C:7]2=[C:8]4[CH:9]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].C(OCC)(=O)C.[OH-].[Na+]>O1CCCC1.O>[Cl:1][C:2]1[CH2:3][N:4]=[CH:5][C:6]2([CH3:21])[CH:17]([CH3:18])[CH:15]3[CH2:16][C:10]4=[C:11]([NH:14]3)[CH2:12][CH2:13][C:7]2=[C:8]4[CH:9]=1

Komponenten

7

Edukt 4

HCID 8857Ethyl AcetateHCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 53643109HCID 53643109, Verbindung

Produkt 1

HCID 73656239HCID 73656239, VerbindungAusbeute 18 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittel2×HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

The nitrile (6.41 g) was dissolved in 300 ml of tetrahydrofuran and, 4.06 g lithium aluminum hydride was added, with stirring. The suspension was heated at reflux for 2 hr and ethyl acetate, water, aqueous sodium hydroxide solution and water were added. The suspension was filtered and the filtrate was concentrated. The residue was triturated with ether and the solid was recrystallized from methanol to give 0.64 g (18%) of the product, mp 260°-263° C. (dec.).

Aufarbeitung

  1. temperatureThe suspension was heated
  2. temperatureat reflux for 2 hr
  3. filtrationThe suspension was filtered
  4. concentrationthe filtrate was concentrated
  5. customThe residue was triturated with ether
  6. customthe solid was recrystallized from methanol

Quellen und Nachweise

ORD-Eintrag
ord-f0157005e31b47d5a5df5ad1ffb1ea49
Quelldatensatz
uspto-grants-1992_09
Patentnummer
US05145965

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